Mixed-wax polyolefin non-flaking coating composition



'tainers for packaging liquids. 'lates to a wax composition having superior non-flaking characteristics, being especially suitable for coating fi- United States Patent 3,173,381 'It EiXED-WAX PflLYOLEFIN NGN-FLAKENG CQFATING CQMPQSHEQN Ivor W; Miils, Glenolden, Pa., and Wilden T. Harvey,

Hockessin, DeL, assignors toSun Gil Company, Philadelphia, Pa, a corporation of New Jersey No Drawing. Filed June 16, 1961, Ser. No. 117,524 SClaims. ((31. 260-285) This'invention relates to a novel wax composition. It particularly relates to a wax composition containing a major 'p'roportion'of a specific parafiin wax, minor proportions of specific microcrystalline wax, another specific paraffin wax, 'a specific polyolefin wax, and a small amount of a specific distillate wax filtrate, the composition being especially suitable for coating fibrous sheets and con- More particularly, it rebrous milk containers.

The use of wax to coat fibrous containers for use in packaging liquids is well known in the art. A particularly useful paratfinwax suitable for coating such containers is described and claimed in United States Patent'No. 2,624,- 501. However, actual commercial use has disclosed several disadvantages of coatings formed from this wax. Suchcoatings on fibrous sheet material may develop minute imperfections which impart a serpentine effect to the coating, thereby creating an unsightly appearance, and leakage of packaged liquid materials through the imperfectionsmayd-evelop. A further difficulty of this wax, as has been found, is the tendency of the coatings formed therefrom to fracture and breakaway from the fibrous material on suifering an impact sonthat wax fia-kes are present in the packaged liquid. Such flaking action of a wax is highly undseirable because the product is rendered objectionable-to ultimate customers.

'An object of the present invention is to provide a wax composition especially suitable for coating fibrous containers for fluids. A particular -object is to provide a wax composition effective for coating paper containers for liquids which imparts a pleasing'appearance to the resulting article of manufacture while providing good coverage and good blocking characteristics and which :can be readily applied withconventional equipment; A specific object is to provide a wax composition which, when formedas a coating for a'fibrous container, will noteasily 'fracture on impact and will have substantially nonrflaking characteristics.

Asusedherein,melting points are determined by ASTM vll)8757, penetrations by ASTM D1i3 2'1-57T, and viscosities (SUSSaybolt Universal Seconds) by ASTM .D446-53, unless otherwise stated. All percentages are weight percent.

T he components of the wax composition of the present invention are characterized as follows;

WAX A This is a relatively low melt-poinrparatlin wax. Typically it has a meltingpoint of from 125 F. to 132 F., a penetration (at 77 F.) of from 17 to 23, a viscosity (at 210 F.) of from 37 to 41 seconds, and a tensilestrength at 40- F. of from 275 psi. to 325 p.s;i., the tensile strength at 40 F. being at least 25 p.s.i. higher than the tensile strength at 70 F. This relatively low melt point paraffin Wax may be prepared as follows: A slack waX from the dewaxing of lubricating oil, which may contain about 30% oil, is vacuum distilled and the fraction dist-illing between about 390 F. and 565 Rat 2 mm. of mercury pressure is collected. This fraction is dissolved in a solvent, preferably a mixture of methyl ethyl ketone and benzene inabout equal volumes. Dissolution is per- "ice formed at an elevatedtemperature, from about 165 F. to 195 F. being suitable, and advantageously about 6 parts by volume of solvent per part of waxis used. The solution is slowly cooled to a temperature of from F. to 83 F. and the wax which precipitates at this temperature is separated such as by filtration. The solution separated from the precipitated wax is further slowly cooled to a temperature of from 28 F. to 33 F. and the wax which precipitates at this temperature is separated and forms Wax A of the present composition. Preferably, the wax after separation from solution is washed, such as with the solvent employed for dissolution, preferably at the same temperature as used for filtration, namely from 28 F. to 32 F. and the wax is then separated.

Analternate method of preparing Wax A of the present invention which provides considerable flexibility in obtaining the desired wax product is ,to separate-from slack wax two distillate fraction, one distilling under vacuum in the range of from about 390 'F. to 475 F. at 2 turn of mercury pressure and a second fraction distilling in the range of from about 450 F. to 565 F. at 2 mm. of mercury pressure. As usually occurs, the initial boiling point of the second fraction will overlap the endpoint of the first-mentioned distilled fraction.- The-lower boiling distillate fraction is dissolved in a solvent as above described and the solut-ionis cooled to a temperature of from 25 F. to 31 F. The wax which precipitates at thistemperature is separated as by filtering. The higher boiling distillate fraction is dissolved in a solvent as above described, except that a lower proportion of solvent to wax, say about 4.5 parts of solventper part ofwax, is advantageously used, and .the solution is slowly cooled to a temperature of from 72 F. to 82 F. The wax which precipitates at this .temperature'is separated such as by filtering and the remaining solution is further slowly cooled to-a tern erature of from 25 F. to 31 F. The wax which precipitates at'this latter temperature is separated as by filtering andis mixed with the wax'recovered from the lower boiling distillate fraction. This mixture of waxes is Wax A of the present invention. Considerable-flexibility is obtainedsince the blending may be in various proportions so that thepropenties of the resulting wax mixture canbe varied within the limits above described for -Wax -A. If desired, the two waxes can be washed and dried'prior to blending, or the wet waxes may be combined and simultaneously washed and then recovered by removal of the wash liquid. In general, from about 60 to 75 pencentby weight of the paraflin wax will comprise wax from the lower boiling distillate-fraction since, as has been--fot1nd,-such mixture gives a wax having properties within .those defined for Wax A of the invention; It is preferred, howeventhat Wax A comprise 75% lower boiling distillate fraction and 25% higher boiling distillate fraction.

WAX B This is a relatively high melt point paratlin wax. Typically it has a melting point of from 148 F. to 154 F., a penetration (at F.) of from 13 to 19 and, a viscosity (at 210 F.) of from 40 to 46 see- This relatively high melting point paraflin' wax may be prepared as follows: A slack wax from the dewaxing of lubricating oilor from topping a high wax content crude oil, is distilled under vacuum, and the fraction distilling in therange of from about 450 F. to 565 F. at 2 mm. of mercury pressure is collected. The distillate fraction is dissolved in a solvent which is preferably a mixture of methyl ethyl ketone and benzene in about equal parts by volume, dissolution advantageously being at a'temperature o'ffrom about F. to F. as above described, using about 2 parts of solvent per part of wax. The solution is slowly cooled to a 3 temperature of from about 77 F. to 83 F. and the wax precipitated at this temperature is separated. The separated wax is washed such as with the solvent employed for dissolution, preferably at the same temperature as used for filtration, and the wax is recovered. This wax forms Wax B of the present invention.

WAX C This is a microcrystalline wax having laminating properties. Typically it has a penetration (at 110 F.) of from 60 to 80, preferably 69 to 74, a viscosity (at 210 F.) of from 70 to 79, and an adhesion value of from 30 to 120, preferably between 65 and 85. The Wax C may be obtained by any of the methods known to the art. One especially suitable method is described and claimed in United States Patent No. 2,783,183. In general, the method of obtaining microcrystalline wax with laminating quality is as follows: A slack wax having from about 20 percent to about 50 percent oil is subjected to vacuum distillation to form a plurality of fractions. The desired fraction is dissolved in a hot solvent, such as a mixture of methyl ethyl ketone and benzene, chilled at one desired temperature and the precipitated wax separated by, say, filtration. The filtrate from this first step is further chilled to another desired lower temperature, and the precipitated wax separated and recovered. This sequence is repeated until the desired wax fraction is obtained.

For example, a microcrystalline wax suitable for use in the composition of this invention is prepared as fol lows: Slack wax containing about 30 percent oil, obtained from the dewaxing of lubricating oils, is continuously vacuum distilled at 650 F. into two distillate fractions, one being removed at about 420 F. at 6 mm. mercury pressure, and the other at about 590 F. at 25 mm. mercury pressure. These low boiling fractions constitute 68 percent of the total charge. The high boiling residual fraction constitutes 32 percent of the total charge and is used for the recovery of the desired microcrystalline wax. This high boiling residual fraction is dissolved in 3.5 parts of a hot (150 F.) solvent mixture comprising 53 percent methyl ethyl ketone and 47 percent benzene. The resulting wax solution is cooled to 93 F., diluted with 5.5 parts of solvent, filtered (or centrifuged) to remove the precipitated wax, and the Wax is washed with 4 parts of solvent. The filtrate from the initial filtrations is further cooled to 58 F., diluted with 6 parts of solvent, filtered, and washed with 4 parts of solvent. The wax product finally obtained, after solvent removal, has an adhesion value between 30 and 120 grams pull per 2 inch width and is designated herein as Wax C.

POLYOLEFIN WAX As used herein, the term polyolefin wax is intended to include the following: low molecular weight polyethylene and low molecular weight isotactic (crystalline) polypropylene.

The polyethylene wax, designated herein as PE, has an average number molecular weight between 1000 and 12,000. Further, a suitable PE has a melt point between about 205 F. and 230 F. and a specific gravity between about 0.900 and 0.930. For example, the PE used herein to illustrate the invention had these properties: average molecular weight, 2000; melt point, 219 F. to 226 F. (ASTM E28-51T); hardness, 3 to (ASTM D1321- SST); specific gravity about 0.92; and viscosity at 40 C. of about 180 centipoises.

The polypropylene wax, designated herein as PP, has an average number molecular weight between 1000 and 12,000 and is characterized by a high degree of crystallinity. A particularly suitable FF is described and claimed in United States Patent No. 2,835,659. However, any commercially available PP which is highly crystalline and within the above-specified molecular weight range can be used satisfactorily in this invention.

Typically, satisfactory PP has a melt point between about 280 F. and 335 F., a specific gravity between about 0.900 and 0.920, and an average molecular weight between about 7000 and 9000.

It is recognized that ethylene and propylene may be copolymerized to a suitable polyolefin wax and used in the wax composition of the invention or PE and PP can be used concurrently as components of said wax composition, or, preferably, may be used separately and individually as component in said wax composition.

DISTILLATE WAX FILTRATE The filtrate component of the present invention, designated herein as DWF, is obtained from a slack Wax fraction boiling within the range of from 360 F. to 580 F. at 2 mm. Hg pressure absolute, and preferably from 400 to 560 F. at 2 mm. Hg pressure absolute. A solvent such as a mixture of methyl ethyl ketone, benzene and toluene is added to the fraction at an elevated temperature sufiicient to obtain complete dissolution, and the resulting solution is chilled to a temperature of from 30 to 35 F. thereby precipitating a substantial quantity of wax. The precipitated wax is then separated by, say, filtration. The filtrate so obtained, after separation of the solvent such as by distillation, constitutes the filtrate component, DWF, of the present invention.

DWF has a boiling range of from 360 F. to 580 F. at 2 mm. Hg pressure absolute and preferably from 400 F. to 560 F. at 2 mm. Hg pressure absolute, a pour point of about 55 F. to F. and preferably about 750 F., and a viscosity at 210 F. of from 42 to 48 seconds, preferably about 45 seconds.

The above-specified components in specific combination make up the wax composition of the present invention. The incorporation of these components into the wax composition can be by any convenient means, such as by blending the waxes in molten state together with the filtrate and the solid polymer, to obtain a homogeneous blend.

The solvent designated in the methods of preparing the wax components may be any of the known dewaxing and deoiling solvents. The preferred solvent is a mixture of methyl ethyl ketone and benzene. Either of the components of the solvent may be replaced, however, in whole or in part, by other ketones, such as methyl butyl ketone or acetone, or hydrocarbons or halogenated hydrocarbons such as ethylene dichloride, pentane, and hexane, or alcohols such as propyl or the heptyl alcohols.

The adhesion test used herein for the microcrystalline wax component is performed as follows: The strips of glassine paper, 2 inches by 6 inches, are laminated with the wax under test by pressing them mildly on a hot plate at a temperature just above the melting point of the wax. The load is adjusted to about 8 pounds of wax per ream of laminate, evenly distributed between the strips. This laminate is held at 73 F. in an atmosphere of 50 percent relative humidity for one hour before testing. Adhesion is the grams pull per 2 inch width required to separate the strips by peeling.

Laminating waxes of the microcrystalline type will have adhesion values, measured as described above, of from 30 to 120. Typtical samples of microcrystalline waxes were tested and the following adhesion values were obtained: 35, 49, 59, 62, 74, 84, 89, 99 and 117.

The Tinius-Olsen angle of fracture test used herein to evaluate the flaking properties of waxes is performed on the Tinius-Olsen Stiffness Tester which has a six pound capacity. The procedure is as follows: Wax is formed into strips of specified dimensions (0.16 inch thick by 0.5 inch wide by 2 inches long) by soldifying molten wax on the surface of water to form the desired thickness, and cutting to the other dimensions. After conditioning at test temperature, these wax strips are placed in the Tinius-Olsen Stiffness Tester and are evaluated for angle of fracture at 73 F. and at 36 F. This angle of fraca ture as measured by this apparatus is the angle at which the specimen fractures. Thus, it is desirable to formulate a wax composition which will, under test, fracture at a high angle of deformation. An angle of 90 is the maximum deformation that can be measured on this instrument. However, for practical reasons, the maximum angle usually measured is 78. Therefore, the number 78 should'be interpreted as 78+.

The angle of fracture values at 73 F. and-36 F. are necessary for complete definition of flaking properties of the specimen, However, the angle of fracture at 36 F. is the critical value because this temperature corresponds approximately to the refrigeration temperature to which,

\say, milk cartons are exposed. The flaking characteristics are evaluated by determining the grams of wax which flake off per 1000 milk cartons of one quart size, after subjecting the milk cartons to the standard drop test. Accordingly, the amount-offlaking to be expected from a wax composition has been correlated with the angle of fracture at 36 F. as follows:

36 angle Flaking, grams: of fracture O 19+ 3 17 Actual experience has shown that a Wax composition with substantially non-flaking characteristics must have a minimum angle of fracture at 36 F. of 13 and at 73 F. a minimum of 20. On the other hand, the commer- 6 To further show the cr-iticality of component concentration, the following illustrations are presented:

Example I A commercially available paratfin wax having prop erties according to Wax A was tested'for flaking character istics with the following results:

Angle of Fracture Wax A Thus, the relatively low me'lt point parafin wax is extremely poor in flaking characteristics.

Example II A commercially available polyethylene wax having typical properties as disclosed hereinabove was blended into molten Wax A. Upon solidifying and testing, the

following results were obtained:

It is concluded that the addition of polyolefin wax to cially available waxes of the art, such as the wax de- Pafafinm Wax does not materially impfove'fiaking resistscribed in United States Patent No. 2,624,501, will have ancean angle of fracture at 36 F. of about 7 which rep- I resents about 60 grams of wax flaking per 1000 milk Example cartons of one quart size. e u 4,0 A slack Wax distillate fractlon filtrate, DWF, was preg g as used hi 4 5 generafi i pared by distilling-slack waxand collecting the fraction 5* ma 6 to Wax Comp 081 Ions W 16 resu m Wax a boiling from 400 F. to 560 F. at 2 mm. Hg pr ssure mg from 10 grams J i i f i absolute. The fraction was dissolved at an elevated one quart slze' Morfaflpartlculfifly P 1s apph' temperature in a solvent consisting of. 60% by volume cable to Wax czmposltlons Y i-f a l i anglf of methyl ethyl ketone, 25% by volume benzene, and 15% fi g 5 i from 13 to 78 an at 73 by volume toluene. Theresulting solution was chilled to o 33 F. and the precipitated wax separated by filtering. It IS essentlal for purpqses the Present i i Solvent was separated from the filtrate by distillation to the components be combined 1n amounts wlthm t e o prepare the, DWF Component The DWF vhad a pom. lowmg Spemfied ranges" point of 75 F. and a viscosity at.2l0. F. of 45 seconds. This filtrate was blended into Wax A with the following Concentration result: Component: range, percent Wax A 48 to 84 7 KB 5 to 25 Angle of Fracture Z C 10 to 30 WaXA DWF Polyolefin wax 0.5 to 2 DVVF 0.5 to 3 An excellent example of the wax composition of the invention'is a blend of: Thus, DWF blended into only Wax A fails to produce a P substantially non-flaking wax.

ercent WaxA 62.8 Example IV $22 6 5 The following blend illustrates the fact that mixing P 1 th PE and DWF into WaxA does not'produce a substanw; y tially non-flaking wax:

100.0 WaXA PE DWF AngleotFracture The above wax composition had an angle of fracture at 73 F. 36 F. 36 F. of 15 and at 73 F. of 21, which according to the correlation is equivalent to about 6 grams of wax flak- 98 1 1 9 7 ing per 1000 milk cartons. 75

7 Example V Angle of Fracture Wax A PE Wax C Example VI The further addition of a relatively high melt point paraflin wax, Wax B, as follows, does markedly improve the 73 F. flexibility but only marginally improves the 36 F. flaking characteristics:

Angle of Fracture Wax A PE Wax C Wax B It is noticed that there is a substantial improvement in the angle of fracture at 73 F. (from 13 to 78+) but only slight improvement at 36 F. (from 8 to an average of about 11).

Example VII The substitution of DWF for PE in a composition similar to that in Example VI has a detrimental effect on flaking. This is illustrated as follows:

Angle of Fracture Wax A PE DWF Wax O Wax B It is also noticed that PE can be reduced to 1% and not affect flexibility.

Example VIII The benefit obtained by using the composition of the present invention is illustrated in the following blends. A distillate wax filtrate, DWF, prepared as in Example III was blended into a mixture of Wax A, Wax B, Wax C, and PE having an average molecular weight of 2000 with the following results:

It is noted that these blends generally have significant improvement in the 36 F. angle of fracture when compared to the previous examples, and all blends are substantially non-flaking.

8 Example IX Increasing the amount of PE from 1% to 2% and varying the Wax B component had the following effect:

Angle of Fracture Wax A Wax B Wax 0 PE DWF It is noted that the 56% Wax A blend is an excellent nonflaking composition. According to the correlation, a 16 angle of fracture at 36 F. is equivalent to about 4 grams of wax flaking per 1000 milk cartons. It is further noted that the specified minimum 73 F. angle of fracture (at least 20) will not be obtained unless the Wax B component is between 20% and 25% of the blend composition. Accordingly, it is concluded that at least 15% Wax B should be used to blend a substantially non-flaking wax composition.

Therefore, according to this invention a wax composition having substantially non-flaking characteristics must comprise essentially from 40% to 84% of parafiin wax having a melt point between 125 F. and 132 F., viscosity at 210 F. of between 37 and 41 seconds, and a tensile strength at 40 F. of from 275 p.s.i. to 325 p.s.i., the tensile strength at 40 F. being at least 25 p.s.i. higher than the tensile strength at 70 F; from 5% to 25% parafiin wax having a melt point between 148 F. and 154 F., viscosity at 210 F. of from 40 to 46 seconds, and a penetration at F. of from 13 to 19; from 10% to 30% microcrystalline wax having a penetration at F. of from 60 to 80, a viscosity at 210 F. of from 70 to 79 seconds, and an adhesion value of from 30 to from 0.5% to 2% polyolefin wax selected from the group consisting of polypropylene and polyethylene; and from. 0.5% to 3% of slack wax distillate fraction filtrate boiling mainly within the range 360 F. to 580 F. at 2 mm. Hg pressure absolute, having a pour point of from 55 F. to 80 F., and having a viscosity at 210 F. of from 42 to 48 seconds; said wax composition having a Tinius-Olsen angle of fracture at 36 F. of at least 13 and at 73 F. of at least 20.

On storing wax slabs prepared from the composition of the present invention for long periods of time under ambient temperature conditions, which includes a temperature of about 90 F., no blocking of the slabs is observed.

The present wax composition is primarily intended for use in coating fibrous fluid containers, particularly cardboard milk containers, which may be advantageously accomplished by dipping or spraying the containers in or with the molten wax. The present wax composition may be used in many other applications, especially where high tensile strength and low temperature flexibility and adherence is desirable, such as in the coating of metal fluid containers, canvas impregnation, coated paper drinking cups, etc.

Furthermore, it is recognized that the wax composition of the present invention may have added thereto various additives, such as antioxidants in amounts ranging from 0.0015% to 2.0%. Certain amides may also be incorporated, for example, to reduce frictional drag of a wax coated milk carton moving through conventional packaging equipment.

We claim:

1. A wax composition comprising essentially from 40% to 84% of paraflin wax having a melt point between F. and 132 F., viscosity at 210 F. of between 37 and 41 seconds, and a tensile strength at 40 F. of from 275 p.s.i. to 325 p.s.i., the tensile strength at 40 F. being at least 25 p.s.i. higher than the tensile strength at 70 F.;

from to paraflin wax having a melt point between 148 F. and 154 F., viscosity at 210 F. of from to 46 seconds, and a penetration at 100 F. of from 13 to 19; from 10% to 30% microcrystalline wax having a penetration at 110 F. of from to 80, a viscosity at 210 F. of from to 79 seconds, and an adhesion value of from 30 to 120; from 0.5% to 2% polyolefin wax selected from the group consisting of isotactic polypropylene and polyethylene; and from 0.5% to 3% of slack wax distillate fraction filtrate boiling mainly within the range 360 F. to 580 F. at 2 mm. Hg pressure absolute, having a pour point of from 55 F. to' 80 F; and having a viscosity at 210 F. of from 42 to 48 seconds; said wax composition having a Tinius-Olsen angle of fracture at 36 F. of at least 13 and at 73 F. of at least 20.

2. A wax composition according to claim 1 wherein said polyolefin wax is polyethylene. V

3. A container for packaging liquids formed from fibrous sheet material and provided with an adherent nonflaking moisture resistant coating, said coating being a hydrocarbon composition comprising essentially from 40% to 84% of parafiin wax having a melt pointbetween 125 F. and 132 F., viscosity at 210 F. of between 37 and 41 seconds, and a tensile strength at 40 F. of from 275 p.s.i. to 325 p.s.i., the tensile strength at 40 F. being at least 25 p.s.i. higher than the tensile strength at 70 F.; from 5% to 25% parafiin wax having a melt point be- 10 tween 148 F. and 154 F., viscosity at 210 F. of from 40 to 46 seconds, and a penetration at F. of from 13 to 19; from 10% to 30% microcrystalline Wax having a penetration at F. of from 60 to 80, a viscosity at 210 F. of from 70 to 79 seconds, and an adhesion value of from 30 to from 0.5% to 2% polyolefin wax selected from the group consisting of isotactic polypropylene and polyethylene; and from 0.5% to 3% of slack Wax distillate fraction filtrate boiling mainly within the range 360 F. to 580 F. at 2 mm. Hg pressure absolute, having a pour point of from 55 F, to 80 F., and having a viscosity at 210 F. of from 42 to 48 seconds; said wax composition having a Tinius-Olsen angle of fracture at 36 F. of at least 13 and at 73 F. of at least 20.

4. A container according to claim 3 wherein said polyolefin wax is polyethylene. V

5 A container according to claim 4 wherein said liquid is milk.

References Cited by the Examiner UNITED STATES PATENTS 2,791,569 5/57 Backlund 260--28.5 2,988,528 6/61 Tench et a1 26028.5

MORRIS LIEBMAN,- Primary Examiner.

MILTON STERMAN, Examiner. 

1. A WAX COMPOSITION COMPRISING ESSENTIALLY FROM 40% TO 84% OF PARAFFIN WAX HAVING A MELT POINT BETWEEN 125* F. AND 132*F., VISCOSITY AT 210*F. OF BETWEEN 37 AND 41 SECONDS, AND A TENSILE STRENGTH AT 40*F. OF FROM 275 P.S.I. TO 325 P.S.I., THE TENSILE STRENGTH AT 40*F. BEING AT LEAST 25 P.S.I. HIGHER THAN THE TENSILE STRENGTH AT 70*F.; FROM 5% TO 25% PARAFFIN WAX HAVING A MELT POINT BETWEEN 148*F. AND 154*F., VISCOSITY AT 210*F OF FROM 40 TO 46 SECONDS, AND A PENETRATION AT 100*F. OF FROM 13 TO 19; FROM 10% TO 30% MICROCRYSTALLINE WAX HAVING A PENETRATION AT 110*F. OF FROM 60 TO 80, A VISCOSITY AT 210*F. OF FROM 70 TO 79 SECONDS, AND AN ADHESION VALUE OF FROM 30 TO 120; FROM 0.5% TO 2% POLYOLEFIN WAX SELECTED FROM THE GROUP CONSISTING OF ISOTACTIC POLYPROPYLENE AND POLYETHYLENE; AND FROM 0.5% TO 3% OF SLACK WAX DISTILLATE FRACTION FILTRATE BOILING MAINLY WITHIN THE RANGE 360*F. TO 580*F. AT 2MM. HG PRESSURE ABSOLUTE, HAVING A POUR POINT OF FROM 55*F. TO 80*F., AND HAVING A VISCOSITY AT 210*F. OF FROM 42 TO 48 SECONDS; SAID WAX COMPOSITION HAVING A TINIUS-OLSEN ANGLE OF FRACTURE AT 36*F. OF AT LEAST 13* AND AT 73*F. OF AT LEAST 20*. 